EP1199393A2 - Method of producing a microfibre, nonwoven with improved liquid-repellent properties - Google Patents

Method of producing a microfibre, nonwoven with improved liquid-repellent properties Download PDF

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Publication number
EP1199393A2
EP1199393A2 EP01122589A EP01122589A EP1199393A2 EP 1199393 A2 EP1199393 A2 EP 1199393A2 EP 01122589 A EP01122589 A EP 01122589A EP 01122589 A EP01122589 A EP 01122589A EP 1199393 A2 EP1199393 A2 EP 1199393A2
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Prior art keywords
microfibers
filler particles
filler
average diameter
diameter
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German (de)
French (fr)
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EP1199393A3 (en
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Sandler AG
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SANDLER C H GmbH
Sandler AG
Christian Heinrich Sandler GmbH and Co KG
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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326Condensation or reaction polymers
    • D04H1/435Polyesters
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43838Ultrafine fibres, e.g. microfibres
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282Addition polymers
    • D04H1/4291Olefin series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326Condensation or reaction polymers
    • D04H1/4334Polyamides
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments

Definitions

  • microfiber nonwovens according to the meltblowing process, described for example in DE 23 08 242, from polyolefinic polymers leads to Microfiber nonwovens with an inherent hydrophobicity. This is due to the hydrophobic properties of the polymers used, such as for example polyethylene or polypropylene.
  • This hydrophobicity is for certain uses, such as in Hygienic nonwovens for backsheet nonwovens and topsheet applications for Panty liners or in the technical application area for roofing membranes and filters which liquid-repellent properties are required are not sufficient.
  • a disadvantage of these methods is that, due to the introduction of the OAS in the polymer, part of the OAS is not actively available on the surface because they are masked in the cooled polymer melt.
  • the task is therefore to develop a process for the production of microfiber nonwovens to provide the OAS used, despite the addition as a master batch, forcibly brought to the surface of the microfibers without being masked Shares of the OAS is coming.
  • the average fiber diameter of the fiber matrix (1) average diameter of the OAS introduced as filler particles (2) adjusted that the average fiber diameter is smaller than the average Diameter of the filler particles (2).
  • values for the middle are preferred Fiber diameter of 0.8 - 0.9 times the average diameter of the Filler.
  • Average diameters of the fiber matrix (1) from including 0.5 to 1.0 times the diameter of the Filler particles (2).
  • An average fiber diameter of less than 0.5 times the diameter the filler particle (2) causes the fiber matrix (1) to tear off Filler particles (2), so that the microfiber nonwoven obtained is mechanically unstable and for the intended purposes as a top sheet or roofing membrane cover is no longer suitable.
  • Fiber diameter of the fiber matrix (1) greater than 1.0 times the Diameter of the filler particles (2) are covered by the prior art.
  • filler particles (2) with an almost monodisperse grain size distribution has proven to be advantageous.
  • the grain size distribution can be determined using the scattering of the Assess grain size diameter. In doing so, distributions of grain sizes are included a standard deviation of less than 3% of the mean found as classified as monodispersed. They are therefore suitable for this process.
  • filler particles (2) come hydrophobic materials from the series Polytetrafluorethylene, the polysiloxanes or the silanes are used. Is not it possible to obtain these active substances in monodisperse form, they can also on carrier substances such as ceramic base materials or on silica be upset.
  • melt flow index of the underlying polymer is also of of great importance for the process.
  • Example 3 the temperature of the Extruder / die (3) increases to increase the viscosity of the polymer melt reduce.
  • Stretching of the fiber stream emerging from the nozzle (3) is intensified in such a way that fiber diameters are set which almost match those of the filler particles correspond. Due to the strongly hydrophobic nature of the used
  • the filler particle (2) now still breaks the filler particle (2) liquid polymer film of the fiber matrix (1) and partially pulls away from the Back surface of the filler particles (2).
  • the cooling unit (4) following the nozzle (3) sprays For example, water as a coolant, causing the fiber matrix to cool quickly (1) leads. However, this remains on part of the surface of the Filler particles (2) stick, but leaves a large part of this surface, as in FIG. 2 shown, but free.
  • the distance (5) of the cooling unit (4) from the central axis of the nozzle (3) is so to choose that cooling at the moment of the above The polymer film breaks open.
  • a nonwoven fabric produced by the method according to the invention shows microscopic observation shows a pearl cord-like structure (FIG. 2), Structures reminiscent of linear ball bearings were also observed.
  • the liquid-repellent effect can be measured using the Hydrohead test made. This test is described in Federal Test Standard No. 191 A, Method 5514, using the nonwoven pattern as the lower seal of a Plastic tube with a diameter of 76 mm is used. In the plastic tube then poured in distilled water until the water passed through the test sample Nonwoven penetrates. The higher the amount of water until penetration, measured in mm, the more hydrophobic is the pattern examined.
  • the spreading is determined by a test, which is a structure liquid-impermeable underlay, in the middle an absorbent body and as an upper one The top sheet provides for the location. On this test setup, 5 ml Blood replacement fluid is given within 20 seconds and the flat Spread this judged on the topsheet in mm. Large area spread is equate with low liquid-repellent properties, the smaller the areal spread is, the greater the liquid rejection.
  • Microfiber nonwovens with an addition of OAS within the melt shows this decrease with repeated wetting not, but, due to the masking of the OAS recognizable from FIG. 1, higher quantities.
  • Microfiber nonwovens such as Example 4 from Table 1, which according to the invention Processes produced do not show this masking effect.

Abstract

In a process for increasing the hydrophobicity of microfibers in a fleece containing polyolefin, polyester or polyamide microfibers with an average diameter of 1-10 mu m, which contain 0.5-10 wt.% firmly embedded filler particles to impart hydrophobicity, the novelty is that the microfibers are produced with an average diameter at most 1.0 times that of the filler particles.

Description

Stand der TechnikState of the art

Die Herstellung von Mikrofaservliesstoffen gemäß dem Schmelzblasverfahren, beispielweise beschrieben in DE 23 08 242, aus polyolefinen Polymeren führt zu Mikrofaser-Vliesstoffen mit einer sich zwangsweise ergebenden Hydrophobie. Diese ist bedingt durch die hydrophoben Eigenschaften der eingesetzten Polymere, wie beispielsweise Polyethylen oder Polypropylen.The production of microfiber nonwovens according to the meltblowing process, described for example in DE 23 08 242, from polyolefinic polymers leads to Microfiber nonwovens with an inherent hydrophobicity. This is due to the hydrophobic properties of the polymers used, such as for example polyethylene or polypropylene.

Diese Hydrophobie ist für bestimmte Einsatzzwecke, wie beispielsweise bei Hygienevliesstoffen für Backsheetvliese und Topsheet-Anwendungen für Slipeinlagen oder im technischen Anwendungsbereich für Dachbahnen und Filter bei welchen flüssigkeitsabweisende Eigenschaften gefordert sind, nicht ausreichend.This hydrophobicity is for certain uses, such as in Hygienic nonwovens for backsheet nonwovens and topsheet applications for Panty liners or in the technical application area for roofing membranes and filters which liquid-repellent properties are required are not sufficient.

Sie muss daher durch entsprechende Behandlungsverfahren auf ein Maß gesteigert werden, dass die so hergestellten Produkte für die späteren Einsatzzwecke geeignet sind. It must therefore be increased to an appropriate level through appropriate treatment procedures that the products manufactured in this way are suitable for later use are.

Dafür sind verschiedene Verfahren bekannt:Various methods are known for this:

Nach Herstellung des Mikrofaservliesstoffes kann beispielsweise mit dem Kühlaggregat Wasser mit einer darin enthaltenen oberflächenaktiven Substanz (OAS) auf den Vliesstoff aufgesprüht werden. Dies wird beispielsweise beschrieben in E.Vargas, Hrsg, "Meltblown Technology Today", Miller Freeman Publications, 1989, Seite 9 , 2. AbsatzAfter production of the microfiber nonwoven, for example, with the Cooling unit water with a surface-active substance contained therein (OAS) are sprayed onto the nonwoven. This is described, for example in E. Vargas, ed., "Meltblown Technology Today", Miller Freeman Publications, 1989, page 9, 2nd paragraph

Diese Methode bringt befriedigende Effekte, und kann die meisten OAS, auch solche mit geringen Temperaturbeständigkeiten, verwenden, hat aber den entscheidenden Nachteil, dass die OAS nur oberflächlich aufliegt und somit nicht beständig gegen Auswaschprozesse ist. Bei hohen Produktionsgeschwindigkeiten führt dieses Verfahren zu ungleichmäßigem Auftrag der OAS. Auch ist ein Abschmieren der OAS bei weiterführenden Verarbeitungsprozessen an Umlenkwalzen gegeben. Es muss daher mehr OAS als zum Erreichen der flüssigkeitsabweisenden Eigenschaften notwendig wäre, eingesetzt werden.This method has satisfactory effects, and can do most OAS, including those with low temperature resistance, but has the decisive one Disadvantage that the OAS is only superficial and therefore not resistant to Washout process is. This leads to high production speeds Procedure for uneven application of the OAS. Lubricating is also the OAS given further processing processes on deflection rollers. It must therefore more OAS than to achieve the liquid-repellent properties would be necessary to be used.

Durch die Entwicklung temperaturbeständiger OAS aus der Reihe der Fluorcarbone ist es möglich, diese Substanzen dem Polymergranulat bereits vor dem Verspinnen als Masterbatch zuzusetzen, sodaß diese während des Aufschmelzens im Extruder homogen in der Polymerschmelze verteilt werden. Die Passage von Extruder und Spinndüse überstehen diese OAS ohne wesentliche Beeinträchtigungen der Eigenschaften durch die dort herrschenden Temperaturen. Mögliche Verfahrenswege hierfür sind in WO 97/43470 A1 oder DE 199 03 663 A1 beschrieben.By developing temperature-resistant OAS from the range of fluorocarbons it is possible to add these substances to the polymer granulate before spinning add as a masterbatch so that it melts in the extruder be distributed homogeneously in the polymer melt. The passage of extruder and Spinning nozzle survive these OAS without significant impairment of the Properties due to the temperatures prevailing there. Possible procedures this is described in WO 97/43470 A1 or DE 199 03 663 A1.

Nachteilig bei diesen Verfahren ist, dass, bedingt durch das Einbringen der OAS in das Polymer, ein Teil der OAS nicht aktiv an der Oberfläche zur Verfügung steht, weil sie in der abgekühlten Polymerschmelze maskiert sind.A disadvantage of these methods is that, due to the introduction of the OAS in the polymer, part of the OAS is not actively available on the surface because they are masked in the cooled polymer melt.

Eine Möglichkeit, die OAS an der Außenfläche der durch das Schmelzblas-Verfahren entstehenden Fasern anzureichern, ist in DE 198 19 682 A1 beschrieben. Hier werden sogenannte Mikropulver auf Basis von Tetraflourethylenhomopolymeren eingesetzt, welche die Bestrebung haben, sich an Grenzflächen abzusetzen. Aber auch hier ist ein Teil der OAS, in Abhängigkeit von Abkühlgeschwindigkeit nach dem Ausspinnen, innerhalb der Polymermatrix maskiert und somit inaktiv. Vergleiche hierzu Figur 1.One way to get the OAS on the outside surface is through the meltblowing process Enriching the resulting fibers is described in DE 198 19 682 A1. Here are so-called micropowders based on tetrafluoroethylene homopolymers deployed who strive to settle at interfaces. But here too is part of the OAS, depending on the cooling rate after the Spinning, masked within the polymer matrix and thus inactive. comparisons see Figure 1.

Aufgabetask

Aufgabe ist es daher, ein Verfahren für die Herstellung von Mikrofaser-Vliesstoffen bereitzustellen, welches die eingesetzten OAS, trotz des Zusatzes als Masterbatch, zwangsweise an die Oberfläche der Mikrofasern bringt ohne daß es zu maskierten Anteilen der OAS kommt.The task is therefore to develop a process for the production of microfiber nonwovens to provide the OAS used, despite the addition as a master batch, forcibly brought to the surface of the microfibers without being masked Shares of the OAS is coming.

Die Aufgabe ist gemäß den Merkmalen des Anspruches 1 gelöst. Ausgestaltungen sind in den Ansprüchen 2 bis 7 genannt.The object is achieved according to the features of claim 1. refinements are mentioned in claims 2 to 7.

Bei Mikrofaservliesstoffen, welche nach dem erfindungsgemäßen Verfahren hergestellt werden, wird der mittlere Faserdurchmesser der Fasermatrix (1) dem mittleren Durchmesser der als Füllstoffpartikel (2) einbrachten OAS derartig angepasst, dass der mittlere Faserdurchmesser geringer ist, als der mittlere Durchmesser der Füllstoffpartikel (2).In the case of microfiber nonwovens, which are produced by the process according to the invention are produced, the average fiber diameter of the fiber matrix (1) average diameter of the OAS introduced as filler particles (2) adjusted that the average fiber diameter is smaller than the average Diameter of the filler particles (2).

Bevorzugt werden bei dem erfindungsgemäßen Verfahren Werte für den mittleren Faserdurchmesser vom 0,8 - 0,9-fachen des mittleren Durchmessers der Füllstoffpartikel. Sinnvoll sind mittlere Durchmesser der Fasermatrix (1) vom einschließlich des 0,5 bis einschließlich des 1,0-fachen des Durchmessers der Füllstoffpartikel (2).In the method according to the invention, values for the middle are preferred Fiber diameter of 0.8 - 0.9 times the average diameter of the Filler. Average diameters of the fiber matrix (1) from including 0.5 to 1.0 times the diameter of the Filler particles (2).

Ein mittlerer Faserdurchmesser von kleiner als dem 0,5-fachen des Durchmessers der Füllstoffpartikel (2) führt zum Abreißen der Fasermatrix (1) von den Füllstoffpartikeln (2), sodaß der erhaltene Mikrofaservliesstoff mechanisch instabil wird und für die vorgesehenen Einsatzzwecke als Topsheet oder Dachbahnabdeckung nicht mehr geeignet ist.An average fiber diameter of less than 0.5 times the diameter the filler particle (2) causes the fiber matrix (1) to tear off Filler particles (2), so that the microfiber nonwoven obtained is mechanically unstable and for the intended purposes as a top sheet or roofing membrane cover is no longer suitable.

Faserdurchmesser der Fasermatrix (1) von größer dem 1,0-fachen des Durchmessers der Füllstoffpartikel (2) sind vom Stand der Technik abgedeckt. Fiber diameter of the fiber matrix (1) greater than 1.0 times the Diameter of the filler particles (2) are covered by the prior art.

Die erfindungsgemäßen Verhältnisse vom Durchmesser der Fasermatrix (1) zum Durchmesser der Füllstoffpartikel (2) werden durch die folgenden Parameter bestimmt:

  • Durchmesser des Füllstoffpartikel (2)
  • Streuung der Durchmesser der Füllstoffpartikel (2)
  • Melt Flow Index des eingesetzten Polymers der Fasermatrix (1)
  • Temperatur im Extruder und der Spinndüse
  • Luftvolumenstrom an der Spinndüse
  • Abstand (5) der Mittelachse der Düse (3) zum Kühlaggregat (4)
The ratios according to the invention of the diameter of the fiber matrix (1) to the diameter of the filler particles (2) are determined by the following parameters:
  • Filler particle diameter (2)
  • Scattering of the diameter of the filler particles (2)
  • Melt Flow Index of the polymer used in the fiber matrix (1)
  • Temperature in the extruder and the spinneret
  • Air volume flow at the spinneret
  • Distance (5) from the central axis of the nozzle (3) to the cooling unit (4)

Zum Einstellen des erfindungsgemäßen Verfahrens haben sich Füllstoffpartikel (2) mit nahezu monodisperser Korngrößenverteilung als vorteilhaft bewährt.To adjust the method according to the invention, filler particles (2) with an almost monodisperse grain size distribution has proven to be advantageous.

Die Korngroßenverteilung lässt sich anhand der Streuung der Korngrößendurchmesser beurteilen. Dabei werden Verteilungen der Korngrößen mit einer Standardabweichung von kleiner 3% vom gefundenen Mittelwert als monodispers verteilt eingestuft. Diese sind daher für diesen Prozess geeignet.The grain size distribution can be determined using the scattering of the Assess grain size diameter. In doing so, distributions of grain sizes are included a standard deviation of less than 3% of the mean found as classified as monodispersed. They are therefore suitable for this process.

Dadurch ist es möglich, Streuungen des Faserdurchmessers weitestgehend zu kompensieren, um die Gefahr der mechanischen Instabilität, besonders bei der Ermittlung des Hydroheads, zu minimieren.This makes it possible to largely reduce scatter in the fiber diameter compensate for the risk of mechanical instability, especially at the Determine the hydrohead to minimize.

Ebenfalls hat es sich als günstig gezeigt, einen Durchmesser der Füllstoffpartikel (2) von 1 µm nicht zu unterschreiten, da es dann zur mechanischen Instabilität des Vliesstoffes aufgrund zu geringer Faserdurchmesser kommt.It has also proven to be advantageous to have a diameter of the filler particles (2) not to fall below 1 µm, since it then leads to mechanical instability of the Nonwoven comes due to insufficient fiber diameter.

Als Füllstoffpartikel (2) kommen hydrophobe Materialien aus der Reihe der Polytetrafluorethylene, der Polysiloxane oder der Silane zum Einsatz. Ist es nicht möglich diese Wirksubstanzen in monodisperser Form zu erhalten, so können diese auch auf Trägersubstanzen wie keramischen Basismaterialien oder auf Kieselsäure aufgebracht sein. As filler particles (2) come hydrophobic materials from the series Polytetrafluorethylene, the polysiloxanes or the silanes are used. Is not it possible to obtain these active substances in monodisperse form, they can also on carrier substances such as ceramic base materials or on silica be upset.

Der Einfluss des Melt Flow Index des zugrundeliegenden Polymers ist ebenfalls von hoher Bedeutung für den Prozess. Je geringer hier die chargeninternen Schwankungen sind, desto gleichmäßiger ist, bei Einhaltung der nachstehend beschriebenen Verfahrensparameter Temperatur und Luftvolumen, der erhaltene mittlere Faserdurchmesser der Fasermatrix (1).The influence of the melt flow index of the underlying polymer is also of of great importance for the process. The lower the batch internal Fluctuations are the more even if the following are observed described process parameters temperature and air volume, the obtained average fiber diameter of the fiber matrix (1).

Für das Erreichen einer erfindungsgemäßen Struktur wie in Figur 2 dargestellt, ist die Temperatur des Extruders und der Düsenspitze in Zusammenhang mit den Luftvolumenströmen der beim Schmelz-Blas Prozess seitlich einströmenden Luft und dem Abstand (5) der Düse (3) vom Kühlaggregat (4) wesentlich.To achieve a structure according to the invention as shown in FIG The temperature of the extruder and the nozzle tip in connection with the Air volume flows of the air flowing in laterally in the meltblowing process and the distance (5) of the nozzle (3) from the cooling unit (4) is essential.

Ausgehend vom Stand der Technik, vergleiche Beispiel 3, wird die Temperatur des Extruders / der Düse (3) erhöht, um die Viskosität der Polymerschmelze zu verringern. Durch gleichzeitige Erhöhung des Luftvolumenstromes wird die Verstreckung des aus der Düse (3) austretenden Faserstroms derart intensiviert, dass sich Faserdurchmesser einstellen welche nahezu denen der Füllstoffpartikel entsprechen. Bedingt durch die stark hydrophobe Natur der eingesetzten Füllstoffpartikel (2) bricht nun der die Füllstoffpartikel (2) umschließende, noch flüssige Polymerfilm der Fasermatrix (1) auf und zieht sich teilweise von der Oberfläche der Füllstoffpartikel (2) zurück.Starting from the prior art, compare Example 3, the temperature of the Extruder / die (3) increases to increase the viscosity of the polymer melt reduce. By simultaneously increasing the air volume flow Stretching of the fiber stream emerging from the nozzle (3) is intensified in such a way that fiber diameters are set which almost match those of the filler particles correspond. Due to the strongly hydrophobic nature of the used The filler particle (2) now still breaks the filler particle (2) liquid polymer film of the fiber matrix (1) and partially pulls away from the Back surface of the filler particles (2).

Wie in Figur 3 aufgezeigt, sprüht das der Düse (3) nachfolgende Kühlaggregat (4) beispielsweise Wasser als Kühlmittel auf, was zum raschen Erkalten der Fasermatrix (1) führt. Dabei bleibt diese aber noch an einem Teil der Oberfläche der Füllstoffpartikel (2) kleben, lässt aber einen Großteil dieser Oberfläche, wie in Figur 2 gezeigt, jedoch frei.As shown in FIG. 3, the cooling unit (4) following the nozzle (3) sprays For example, water as a coolant, causing the fiber matrix to cool quickly (1) leads. However, this remains on part of the surface of the Filler particles (2) stick, but leaves a large part of this surface, as in FIG. 2 shown, but free.

Der Abstand (5) des Kühlaggregats (4) von der Mittelachse der Düse (3) ist dabei so zu wählen, dass das Erkalten in dem Moment des vorstehend beschriebenen Aufbrechens des Polymerfilms einsetzt.The distance (5) of the cooling unit (4) from the central axis of the nozzle (3) is so to choose that cooling at the moment of the above The polymer film breaks open.

Einstellwerte für den Abstand (5) sind von der gegebenen baulichen Maschinenkonfiguration und von den vorstehend beschriebenen Parametern abhängig, sodaß sich dieser nur empirisch ermitteln lässt. Setting values for the distance (5) are of the given structural Machine configuration and the parameters described above dependent, so that this can only be determined empirically.

Ein nach dem erfindungsgemäßen Verfahren hergestellter Vliesstoff zeigt bei mikroskopischer Betrachtung eine perlenschnurartige Struktur (Figur 2) gezeigt, beobachtet wurden aber auch Strukturen, welche an Linearkugellager erinnern.A nonwoven fabric produced by the method according to the invention shows microscopic observation shows a pearl cord-like structure (FIG. 2), Structures reminiscent of linear ball bearings were also observed.

Die Eignung für den gedachten Einsatzzweck wird nach den Ergebnissen von anwendungsspezifischen Tests beurteilt. Nachstehend wird stellvertretend für andere Anwendungen der Bereich Damenhygiene betrachtet.The suitability for the intended application is based on the results of assessed application-specific tests. The following is representative of others Applications in the area of feminine hygiene considered.

Die flüssigkeitsabweisende Wirkung wird mittels des Hydrohead-Tests messbar gemacht. Dieser Test wird nach der Beschreibung in Federal Test Standard No. 191 A, Method 5514 ausgeführt, wobei das Vliesstoff-Muster als untere Abdichtung eines Kunststoffrohres mit einem Durchmesser von 76 mm dient. In das Kunststoffrohr wird dann destilliertes Wasser eingefüllt, bis das Wasser durch den zu testenden Vliesstoff dringt. Je höher dabei die Wassermenge bis zum Durchdringen, gemessen in mm, ist, um so hydrophober ist das untersuchte Muster.The liquid-repellent effect can be measured using the Hydrohead test made. This test is described in Federal Test Standard No. 191 A, Method 5514, using the nonwoven pattern as the lower seal of a Plastic tube with a diameter of 76 mm is used. In the plastic tube then poured in distilled water until the water passed through the test sample Nonwoven penetrates. The higher the amount of water until penetration, measured in mm, the more hydrophobic is the pattern examined.

Eine weitere Methode zur Beschreibung der flüssigkeitsabweisenden Eigenschaften, welche im Bereich der Hygienevliesstoffe, insbesondere bei Topsheet-Anwendungen in der Damenhygiene, zur Anwendung kommt, wird als Spreading bezeichnet.Another method to describe the liquid-repellent properties, which in the field of hygienic nonwovens, especially in topsheet applications in feminine hygiene, is used as spreading.

Das Spreading wird dabei durch einen Test ermittelt, welcher als Aufbau eine flüssigkeitsundurchlässige Unterlage, in der Mitte einen Saugkörper und als obere Lage das Topsheet vorsieht. Auf diesen Testaufbau werden nun 5 ml Blutersatzflüssigkeit innerhalb von 20 Sekunden gegeben und das flächige Ausbreiten dieser auf dem Topsheet in mm beurteilt. Große flächige Ausbreitung ist dabei mit geringen flüssigkeitsabweisenden Eigenschaften gleichzusetzen, je kleiner die flächige Ausbreitung ist, umso größer ist die Flüssigkeitsabweisung.The spreading is determined by a test, which is a structure liquid-impermeable underlay, in the middle an absorbent body and as an upper one The top sheet provides for the location. On this test setup, 5 ml Blood replacement fluid is given within 20 seconds and the flat Spread this judged on the topsheet in mm. Large area spread is equate with low liquid-repellent properties, the smaller the areal spread is, the greater the liquid rejection.

Nach dem Stand der Technik hergestellte Mikrofaservliesstoffe ohne Zusätze, vergleiche Beispiel 1 von Tabelle 1, erreichen, bei einem gemäß EDANA ERT 40.3-90 ermittelten Flächengewicht von 15 g/qm, ein Hydrohead-Ergebnis von 320 mm und Spreading-Werte von 45 mm. State-of-the-art microfiber nonwovens without additives, compare example 1 of table 1, with one according to EDANA ERT 40.3-90 determined basis weight of 15 g / qm, a hydrohead result of 320 mm and spreading values of 45 mm.

Bei Mikrofaservliesstoffen in einem vergleichbaren Flächengewicht, aber mit einem Zusatz von OAS im Kühlwasser wie in Beispiel 2 von Tabelle 1 beschrieben, werden Hydrohead-Ergebnisse von 410 mm und ein Spreading von 37 mm erzielt.For microfiber nonwovens with a comparable basis weight, but with one Add OAS in the cooling water as described in Example 2 of Table 1 Hydrohead results of 410 mm and a spreading of 37 mm achieved.

Wiederholt man die Prüfung, bemerkt man, aufgrund der Eingangs beschriebenen Problematik des Auswaschens/Abreibens der OAS ein drastisches Absinken der flüssigkeitsabweisenden Eigenschaften, sodass sich bei erneuter Prüfung Werte in Höhe der Ergebnisse nicht ausgerüsteter Mikrofaser-Vliesstoffe ergeben.If you repeat the test, you will notice, based on the description described at the beginning Problem of washing out / rubbing the OAS a drastic drop in the liquid-repellent properties, so that when tested again, values in Results of unfinished microfiber nonwovens result.

Mikrofaservliesstoffe mit einem Zusatz von OAS innerhalb der Schmelze, wie in Beispiel 3 von Tabelle 1, zeigen dieses Absinken bei mehrmaliger Benetzung zwar nicht, benötigen aber, aufgrund der aus Figur 1 erkennbaren Maskierung der OAS, höhere Einsatzmengen.Microfiber nonwovens with an addition of OAS within the melt, as in Example 3 of Table 1 shows this decrease with repeated wetting not, but, due to the masking of the OAS recognizable from FIG. 1, higher quantities.

Mikrofaservliesstoffe wie Beispiel 4 aus Tabelle 1, welche nach dem erfindungsgemäßen Verfahren hergestellt werden, zeigen diesen Maskierungseffekt nicht.Microfiber nonwovens such as Example 4 from Table 1, which according to the invention Processes produced do not show this masking effect.

Für die Eigenschaften dieser Mikrofaservliesstoffe bedeutet dies, dass selbst mit geringen Einsatzmengen an OAS im Vergleich zum Stand der Technik, ein Vliesstoff mit höheren flüssigkeitsabweisenden Eigenschaften erzeugt wird. Bei Betrachtung der Tabelle 1 zeigt sich für das Beispiel 4 ein um 35% höherer Hydrohead und ein Spreading, welches 40% unter dem des Standes Technik liegt, wobei die Einsatzmenge an aktiver Wirksubstanz nur 60% der des Beispiels 3 war.For the properties of these microfiber nonwovens, this means that even with small amounts of OAS used compared to the prior art, a nonwoven is produced with higher liquid-repellent properties. On consideration Table 1 shows a 35% higher hydrohead and a for example 4 Spreading, which is 40% below that of the prior art, the The amount of active substance used was only 60% of that of Example 3.

Verfahrenseinstellungen und Ergebnisse erfindungsgemäß hergestellter Mikrofaservliesstoffe im Vergleich zum Stand der Technik können der Tabelle 1 entnommen werden.Process settings and results produced according to the invention Microfiber nonwovens compared to the prior art can be found in Table 1 be removed.

Claims (7)

Verfahren zur Erhöhung der hydrophoben Eigenschaften von Mikrofasern eines Mikrofasern enthaltenden Vliesstoffes, wobei der mittlere Durchmesser der Mikrofasern 1- 10 µm beträgt und die Mikrofasern aus einem Polymeren aus der Gruppe der Polyolefine, oder der Polyester, oder der Polyamide besteht und die hydrophoben Eigenschaften durch mindestens einen, in das Faserpolymere der Mikrofasern fest eingelagerten partikelförmigen, in einer Menge von 0,5 bis 10 Gewichts-% bezogen auf das Gewicht der Mikrofasern vorliegenden festen Füllstoff enthält,
dadurch gekennzeichnet, daß Mikrofasern erzeugt werden deren mittlerer Durchmesser höchstens das 1,0-fache des mittleren Durchmessers der Füllstoffpartikel beträgt.
Process for increasing the hydrophobic properties of microfibers of a nonwoven containing microfibers, the mean diameter of the microfibers being 1-10 μm and the microfibers consisting of a polymer from the group of polyolefins, or of polyesters, or of polyamides, and the hydrophobic properties of at least contains a particulate solid filler which is firmly embedded in the fiber polymers of the microfibers and is present in an amount of 0.5 to 10% by weight, based on the weight of the microfibers,
characterized in that microfibers are produced whose average diameter is at most 1.0 times the average diameter of the filler particles.
Verfahren nach Anspruch 1,
dadurch gekennzeichnet, daß Mikrofasern erzeugt werden deren mittlerer Durchmesser wenigstens das 0,5 -fache des mittleren Durchmessers der Füllstoffpartikel beträgt.
Method according to claim 1,
characterized in that microfibers are produced whose average diameter is at least 0.5 times the average diameter of the filler particles.
Verfahren nach Anspruch 1 und 2
dadurch gekennzeichnet, daß der Füllstoff unvollständig vom Polymeren der Mikrofasern eingeschlossen ist.
The method of claims 1 and 2
characterized in that the filler is incompletely enclosed by the polymer of the microfibers.
Verfahren nach Anspruch 1 bis 2
dadurch gekennzeichnet daß das Füllstoffpartikel durchgehend aus einer hydrophoben Substanz wie Polytertrafluorethylen besteht.
The method of claims 1 to 2
characterized in that the filler particle consists consistently of a hydrophobic substance such as polytertrafluoroethylene.
Verfahren nach Anspruch 1 bis 2
dadurch gekennzeichnet daß die Füllstoffpartikel lediglich oberflächlich mit einer hydrophoben Substanz wie Polytetrafluorethylen, Polysiloxanen oder Silanen versehen sind.
The method of claims 1 to 2
characterized in that the filler particles are only superficially provided with a hydrophobic substance such as polytetrafluoroethylene, polysiloxanes or silanes.
Verfahren nach Anspruch 1 bis 2
dadurch gekennzeichnet daß die Füllstoffpartikel ganz oder lediglich im Kern aus einer anorganischen Substanz wie beispielsweise Keramik oder Kieselsäure bestehen.
The method of claims 1 to 2
characterized in that the filler particles consist entirely or only in the core of an inorganic substance such as ceramic or silica.
Verfahren nach Anspruch 1 bis 2
dadurch gekennzeichnet daß die Füllstoffpartikel aus einer duroplastischen organischen Substanz wie beispielsweise Phenolharz oder Harnstoff-Formaldeydharz bestehen.
Figure 00100001
The method of claims 1 to 2
characterized in that the filler particles consist of a thermosetting organic substance such as phenolic resin or urea-formaldehyde resin.
Figure 00100001
EP01122589A 2000-10-11 2001-09-26 Method of producing a microfibre, nonwoven with improved liquid-repellent properties Withdrawn EP1199393A3 (en)

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RU2668446C1 (en) * 2018-01-16 2018-10-01 Акционерное общество "Научно-исследовательский институт синтетического волокна с экспериментальным заводом" (АО "ВНИИСВ") Installation for obtaining sorption filtering nonwoven materials with improved properties from polymer solutions by method of aerodynamic formation
US10501876B2 (en) 2010-09-14 2019-12-10 Thueringisches Institut Fuer Textil-Und Kunststoff-Forschung E.V. Highly functional spunbonded fabric made from particle-containing fibres and method for producing same

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CN114395808B (en) * 2022-02-21 2023-02-28 季华实验室 Method for preparing polytetrafluoroethylene fiber by wet spinning

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